CA1252705A - Method for analyzing different sulphur forms - Google Patents
Method for analyzing different sulphur formsInfo
- Publication number
- CA1252705A CA1252705A CA000470308A CA470308A CA1252705A CA 1252705 A CA1252705 A CA 1252705A CA 000470308 A CA000470308 A CA 000470308A CA 470308 A CA470308 A CA 470308A CA 1252705 A CA1252705 A CA 1252705A
- Authority
- CA
- Canada
- Prior art keywords
- sulphur
- sample
- coal
- infrared
- combustion
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 14
- 239000005864 Sulphur Substances 0.000 claims abstract description 41
- 239000003245 coal Substances 0.000 claims abstract description 31
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000002485 combustion reaction Methods 0.000 claims abstract description 19
- 235000010269 sulphur dioxide Nutrition 0.000 claims abstract description 9
- 239000004291 sulphur dioxide Substances 0.000 claims abstract description 8
- 239000000567 combustion gas Substances 0.000 claims abstract description 7
- 238000002329 infrared spectrum Methods 0.000 claims abstract description 3
- 239000011159 matrix material Substances 0.000 claims description 5
- 238000012544 monitoring process Methods 0.000 claims 2
- 239000007787 solid Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 4
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical compound [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 description 13
- 229910052683 pyrite Inorganic materials 0.000 description 13
- 239000011028 pyrite Substances 0.000 description 13
- 239000000843 powder Substances 0.000 description 11
- 230000001590 oxidative effect Effects 0.000 description 7
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 229910021653 sulphate ion Inorganic materials 0.000 description 4
- 235000003891 ferrous sulphate Nutrition 0.000 description 3
- 239000011790 ferrous sulphate Substances 0.000 description 3
- 230000001788 irregular Effects 0.000 description 3
- XTQHKBHJIVJGKJ-UHFFFAOYSA-N sulfur monoxide Chemical class S=O XTQHKBHJIVJGKJ-UHFFFAOYSA-N 0.000 description 3
- 241000255964 Pieridae Species 0.000 description 2
- 238000010494 dissociation reaction Methods 0.000 description 2
- 230000005593 dissociations Effects 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- YALHCTUQSQRCSX-UHFFFAOYSA-N sulfane sulfuric acid Chemical compound S.OS(O)(=O)=O YALHCTUQSQRCSX-UHFFFAOYSA-N 0.000 description 2
- 238000003916 acid precipitation Methods 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- 229910000360 iron(III) sulfate Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/12—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using combustion
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/22—Fuels; Explosives
- G01N33/222—Solid fuels, e.g. coal
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T436/00—Chemistry: analytical and immunological testing
- Y10T436/18—Sulfur containing
- Y10T436/182—Organic or sulfhydryl containing [e.g., mercaptan, hydrogen, sulfide, etc.]
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Pathology (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Medicinal Chemistry (AREA)
- Combustion & Propulsion (AREA)
- Molecular Biology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
Abstract:
A method is described for quantitatively determining the different forms of sulphur present in a sample of material, such as coal. The sulphur-containing sample is burned in finely divided form within a confined combustion chamber at a predetermined elevated temperature. Combust-ion gases are continuously removed from the chamber and these pass through an infrared analyzer which continuously monitors the intensity of the infrared spectra for sulphur dioxide in the combustion gases. The infrared intensity is measured as a function of combustion time of the sample to obtain peaks in the infrared intensity-time pattern indicative of different forms of sulphur. From these pattern peaks the quantity of each form of sulphur in the sample is determined.
A method is described for quantitatively determining the different forms of sulphur present in a sample of material, such as coal. The sulphur-containing sample is burned in finely divided form within a confined combustion chamber at a predetermined elevated temperature. Combust-ion gases are continuously removed from the chamber and these pass through an infrared analyzer which continuously monitors the intensity of the infrared spectra for sulphur dioxide in the combustion gases. The infrared intensity is measured as a function of combustion time of the sample to obtain peaks in the infrared intensity-time pattern indicative of different forms of sulphur. From these pattern peaks the quantity of each form of sulphur in the sample is determined.
Description
1 ~Z7'~5 M th d for anal-zin different sul hur forms e o ~ q This invention relates to a method and apparatus for quantitatively determining the different forms of sulphur present in a matrix, such as coal.
One of the more serious environmental problems through-out the world is air pollution due to the emission of sulphur oxides when sulphur-containing fuels are burned.
It is now widely recognized that sulphur oxides are particularly harmful pollutants, producing what is now know as acid rain.
Coal remains one of the world's most important fuel sources and large quantities are burned in thermo-generating plants for conversion into electrical energy.
Many coals contain substantial amounts of sulphur which generate unacceptable amounts of sulphur oxides on burning. Coal combustion is by far the largest single source of sulphur dioxide pollution in the United States.
The sulphur content of coal, nearly all of which is emitted as sulphur dioxides during combustion, is present in essentially three forms: pyritic sulphur, organic sulphur and sulphate sulphur. Distribution between the different forms of sulphur varies widely among various coals and can even vary quite substantially within a single coal deposit.
~4 It is, of course, highly desirable to be able to remove substantial portions of the sulphur present in coal before the coal is burned. Since the different forms of sulphur must be removed by different techniques, how a given supply of coal will be processed will be largely dependent on the relative proportions of the different forms of sulphur present in the coal. The present ASTM methods of analy-zing for the different forms of sulphur present in coal are exceedingly time consuming and require highly trained personnel. For instance, the current practice utilizes wet analysis of pyritic and sulphatic sulphur to get the content of organic sulphur by differe~ce from the total sulphur contents.
There are many different instruments available on the market that can quickly analyze the total sulphur content of coal. For instance, one commercial analyzer oxidizes the coal sample in a resistance furnace, where the sulphur in the coal is combusted to sulphur dioxide gas which is detected by an infrared detector. However, this analyzer is capable only of giving the total infrared intensity, time integrated as the total sulphur content.
It is the object of the present invention to provide a method and apparatus which can quantitatively determine the different forms of sulphur present in a matrix, such as coal, as simply as total sulphurs can now be determined.
Thus, the present invention relates to a method for quantitatively determining the different forms of sulphur present in a sulphur containing material, such as coal, in which a finely divided sulphur-containing sample is burned within a confined combustion chamber. This combustion chamber is at a predetermined elevated temperature, and the combustion gases from the combustion chamber are continuously removed. These removed combustion gases pass through an infrared analyzer which continuously monitors the intensity of the infrared spectra for sulphur dioxide in the combustion gases. The infrared intensity is --3~
measured as a function of evolution time of sulphur - dioxide from the coal sample to obtain peaks in an infrared intensity time pattern indicative of different forms of sulphur. Based upon the shape of these pattern peaks, the quantity of each form of sulphur in the sample can be determined.
In accordance with the present invention, it has been now shown that the different forms of sulphur within coal or other matrix have sufficiently different oxidation or dissociation rates that these can be detected and measured on the basis of sulphur dioxide emissions during oxidation.
The different forms of sulphu~ can be shown as separate and distinct peaks on an infrared spectro-chronogram, Thus, the area under the total curve of such spectro-chronogram represents the total sulphur content of the sample and when the different peaks in the curve are resolved into individual curves, the areas under the individual curves can be identified with the amounts of the different forms of sulphur in the total sample. The multi-peak curve can be resolved înto individual curves by known techniques utilizing microprocessor technology.
~he temperature in the combustion chamber can change the peak positions of the spectro-chronograms, as well as the characteristics or shape of the curves. Thus, the peaks become broader and lower at lower chamber tempera-tures, and with increasing temperatures, the peaks become more sharply defined and the oxidation and/or dissociation kinetics become faster. Preferably the temperature or the combustion chamber is maintained within the range of about 500C to 2000C. Within this general range, an optimum temperature is selected to provided the bes~ definitions of the different components.
It has also been found that it is important that the samples of coal to be analyzed be finely divided and also be in the form of a uniform thin layer. Preferably, the 7~5 samples have particle sizes of minus 10~. This finely divided material is then thinly spread in a uniform layer in a sample container, e.g. a sample boat. Uneven piling of a sample results in an irregular shape to the sprecto-chronogram curve.
A series of experiments were conducted on a modified "LECO SC-32 Sulphur Detector". In the conventional operation of this analyzer, the output of the device (inverse of infrared adsorption intensity for a fixed wavelength of S02~ is collected in the form of digital data to arrive at the total sulphur content of a coal sample. For the present studies, the above analyzer was modified so that the infrared signal output was continuously recorded as a function of oxidizing time to give spectro-chronograms.
In the drawings which illustrate the invention:
Figure 1 is IR spectro-chronograms for S02 from oxidizing pyrite at different temperatures;
Figure 2 is IR spectro-chronograms for S02 from oxidizing different sample sizes of pyrite;
Figure 3 is IR spectro-chronograms for S02 from oxidizing different physical arrangements of pyrite samples;
Figure 4 is IR spectro-chronograms for S02 from oxidizing coal, pyrite, Fe2(S04)3 and FeS04;
Figure 5 is an IR spectro-chronogram for S02 from oxidizing a mixed sample; and Figure 6 is I~ spectro-chronograms for S02 from oxidizing four different coal samples.
The following examples are provided to more specifically illustrate the inven~ion described herein.
Example 1 A series of tests were conducted on a sample of pyrite using the above modified analyzer. These tests were to determine the affects of combustion chamber temperatures on the spectro-chronogram curves.
~2~05 Powders of pure pyrite were placed in sample boats and analyzed within the modified analyzer at combustion chamber temperatures ranging between 598C and 1038C. The results are shown Figure 1 and it will be seen that with increasing temperatures, the peaks became more sharply defined and the oxidation kinetics became faster.
Since a 2 mg sample of pyrite was used in each test, the areas under the curves for ~he different temperatures remain unchanged. In other words, the peak became broader and lower at the lower temperature.
Example 2 Following the same general pro~edu~e as in Example 1, pure pyrite powder samples of different sizes varying between 1 mg and 20 mg were oxidized. The combustion chamber was maintained at 954C for e~ach test.
The results are shown in Figure 2 and it will be seen that the area under each curve is proportional to the amount of sample used. The peak positions remained constant at about 65 seconds under the chosen experimental conditions. The peaks became higher and broader with increasing amounts of samples.
Example 3 Again following the same general procedures as in the previous examples, two samples of pure pyrite powder were oxidized at 954C. However, one sample was placed as an irregular pile in a sample boat while the other sample was spread evenly across the bottom of a sample boat. As will be seen from Figure 3, uneven piling of the sample resulted in an irregular shape of the curve.
Example 4 Tests were conducted on samples of coal powder, pure pyrite powder, pure ferrous sulphate powder and pure ferric sulphate powder at a combustion chamber temperature of 1149C. The results of these tests are shown in Figure 4 and it will be seen tha~ the sulphur in the coal oxidized 1~5~ S
faster than that in pyrite. The breakdown of the sulphate iron into sulphur dioxide occurred much later than pyrite and the ferric sulphate dissociated a little slower than ferrous sulphate, reflecting the difference in the bond strength.
Example 5 A mixed sample was prepared consisting of 50.2 mg coal powder, 2.0 mg pure pyrite powder, 20.6 mg pure ferrous sulphate powder and 10.6 mg ferric sulphate powder. This sample was oxidized in the modified analyzer at a combus~ion chamber temperature of 1149C. The results obtained are shown in Figure 5. A complex curve was obtained but the distinct peaks representative of the different sulphur forms are clearly visible.
Example 6 For this test, a series of different standard coal samples were used containing different amounts of organic, pyritic and sulphate sulphur.
Four different coal samples were oxidized in the above modified analyzer at a combustion chamber temperature of 1038C and the results obtained are shown in Figure 6. It will be seen that the four curves differ widely in characteristics and these differences are based upon the different amounts of organic, pyritic and sulphate sulphurs present in the different samples.
Having thus described the present invention, it should be noted that various other alternatives, adaptations and modifications may be used within the scope of the present invention. For instance, while the description relates primarily to the detection of different forms of sulphur present in coal, the sulphur being detected may be present in many materials other than coal.
One of the more serious environmental problems through-out the world is air pollution due to the emission of sulphur oxides when sulphur-containing fuels are burned.
It is now widely recognized that sulphur oxides are particularly harmful pollutants, producing what is now know as acid rain.
Coal remains one of the world's most important fuel sources and large quantities are burned in thermo-generating plants for conversion into electrical energy.
Many coals contain substantial amounts of sulphur which generate unacceptable amounts of sulphur oxides on burning. Coal combustion is by far the largest single source of sulphur dioxide pollution in the United States.
The sulphur content of coal, nearly all of which is emitted as sulphur dioxides during combustion, is present in essentially three forms: pyritic sulphur, organic sulphur and sulphate sulphur. Distribution between the different forms of sulphur varies widely among various coals and can even vary quite substantially within a single coal deposit.
~4 It is, of course, highly desirable to be able to remove substantial portions of the sulphur present in coal before the coal is burned. Since the different forms of sulphur must be removed by different techniques, how a given supply of coal will be processed will be largely dependent on the relative proportions of the different forms of sulphur present in the coal. The present ASTM methods of analy-zing for the different forms of sulphur present in coal are exceedingly time consuming and require highly trained personnel. For instance, the current practice utilizes wet analysis of pyritic and sulphatic sulphur to get the content of organic sulphur by differe~ce from the total sulphur contents.
There are many different instruments available on the market that can quickly analyze the total sulphur content of coal. For instance, one commercial analyzer oxidizes the coal sample in a resistance furnace, where the sulphur in the coal is combusted to sulphur dioxide gas which is detected by an infrared detector. However, this analyzer is capable only of giving the total infrared intensity, time integrated as the total sulphur content.
It is the object of the present invention to provide a method and apparatus which can quantitatively determine the different forms of sulphur present in a matrix, such as coal, as simply as total sulphurs can now be determined.
Thus, the present invention relates to a method for quantitatively determining the different forms of sulphur present in a sulphur containing material, such as coal, in which a finely divided sulphur-containing sample is burned within a confined combustion chamber. This combustion chamber is at a predetermined elevated temperature, and the combustion gases from the combustion chamber are continuously removed. These removed combustion gases pass through an infrared analyzer which continuously monitors the intensity of the infrared spectra for sulphur dioxide in the combustion gases. The infrared intensity is --3~
measured as a function of evolution time of sulphur - dioxide from the coal sample to obtain peaks in an infrared intensity time pattern indicative of different forms of sulphur. Based upon the shape of these pattern peaks, the quantity of each form of sulphur in the sample can be determined.
In accordance with the present invention, it has been now shown that the different forms of sulphur within coal or other matrix have sufficiently different oxidation or dissociation rates that these can be detected and measured on the basis of sulphur dioxide emissions during oxidation.
The different forms of sulphu~ can be shown as separate and distinct peaks on an infrared spectro-chronogram, Thus, the area under the total curve of such spectro-chronogram represents the total sulphur content of the sample and when the different peaks in the curve are resolved into individual curves, the areas under the individual curves can be identified with the amounts of the different forms of sulphur in the total sample. The multi-peak curve can be resolved înto individual curves by known techniques utilizing microprocessor technology.
~he temperature in the combustion chamber can change the peak positions of the spectro-chronograms, as well as the characteristics or shape of the curves. Thus, the peaks become broader and lower at lower chamber tempera-tures, and with increasing temperatures, the peaks become more sharply defined and the oxidation and/or dissociation kinetics become faster. Preferably the temperature or the combustion chamber is maintained within the range of about 500C to 2000C. Within this general range, an optimum temperature is selected to provided the bes~ definitions of the different components.
It has also been found that it is important that the samples of coal to be analyzed be finely divided and also be in the form of a uniform thin layer. Preferably, the 7~5 samples have particle sizes of minus 10~. This finely divided material is then thinly spread in a uniform layer in a sample container, e.g. a sample boat. Uneven piling of a sample results in an irregular shape to the sprecto-chronogram curve.
A series of experiments were conducted on a modified "LECO SC-32 Sulphur Detector". In the conventional operation of this analyzer, the output of the device (inverse of infrared adsorption intensity for a fixed wavelength of S02~ is collected in the form of digital data to arrive at the total sulphur content of a coal sample. For the present studies, the above analyzer was modified so that the infrared signal output was continuously recorded as a function of oxidizing time to give spectro-chronograms.
In the drawings which illustrate the invention:
Figure 1 is IR spectro-chronograms for S02 from oxidizing pyrite at different temperatures;
Figure 2 is IR spectro-chronograms for S02 from oxidizing different sample sizes of pyrite;
Figure 3 is IR spectro-chronograms for S02 from oxidizing different physical arrangements of pyrite samples;
Figure 4 is IR spectro-chronograms for S02 from oxidizing coal, pyrite, Fe2(S04)3 and FeS04;
Figure 5 is an IR spectro-chronogram for S02 from oxidizing a mixed sample; and Figure 6 is I~ spectro-chronograms for S02 from oxidizing four different coal samples.
The following examples are provided to more specifically illustrate the inven~ion described herein.
Example 1 A series of tests were conducted on a sample of pyrite using the above modified analyzer. These tests were to determine the affects of combustion chamber temperatures on the spectro-chronogram curves.
~2~05 Powders of pure pyrite were placed in sample boats and analyzed within the modified analyzer at combustion chamber temperatures ranging between 598C and 1038C. The results are shown Figure 1 and it will be seen that with increasing temperatures, the peaks became more sharply defined and the oxidation kinetics became faster.
Since a 2 mg sample of pyrite was used in each test, the areas under the curves for ~he different temperatures remain unchanged. In other words, the peak became broader and lower at the lower temperature.
Example 2 Following the same general pro~edu~e as in Example 1, pure pyrite powder samples of different sizes varying between 1 mg and 20 mg were oxidized. The combustion chamber was maintained at 954C for e~ach test.
The results are shown in Figure 2 and it will be seen that the area under each curve is proportional to the amount of sample used. The peak positions remained constant at about 65 seconds under the chosen experimental conditions. The peaks became higher and broader with increasing amounts of samples.
Example 3 Again following the same general procedures as in the previous examples, two samples of pure pyrite powder were oxidized at 954C. However, one sample was placed as an irregular pile in a sample boat while the other sample was spread evenly across the bottom of a sample boat. As will be seen from Figure 3, uneven piling of the sample resulted in an irregular shape of the curve.
Example 4 Tests were conducted on samples of coal powder, pure pyrite powder, pure ferrous sulphate powder and pure ferric sulphate powder at a combustion chamber temperature of 1149C. The results of these tests are shown in Figure 4 and it will be seen tha~ the sulphur in the coal oxidized 1~5~ S
faster than that in pyrite. The breakdown of the sulphate iron into sulphur dioxide occurred much later than pyrite and the ferric sulphate dissociated a little slower than ferrous sulphate, reflecting the difference in the bond strength.
Example 5 A mixed sample was prepared consisting of 50.2 mg coal powder, 2.0 mg pure pyrite powder, 20.6 mg pure ferrous sulphate powder and 10.6 mg ferric sulphate powder. This sample was oxidized in the modified analyzer at a combus~ion chamber temperature of 1149C. The results obtained are shown in Figure 5. A complex curve was obtained but the distinct peaks representative of the different sulphur forms are clearly visible.
Example 6 For this test, a series of different standard coal samples were used containing different amounts of organic, pyritic and sulphate sulphur.
Four different coal samples were oxidized in the above modified analyzer at a combustion chamber temperature of 1038C and the results obtained are shown in Figure 6. It will be seen that the four curves differ widely in characteristics and these differences are based upon the different amounts of organic, pyritic and sulphate sulphurs present in the different samples.
Having thus described the present invention, it should be noted that various other alternatives, adaptations and modifications may be used within the scope of the present invention. For instance, while the description relates primarily to the detection of different forms of sulphur present in coal, the sulphur being detected may be present in many materials other than coal.
Claims (5)
1. A method for quantitatively determining the different forms of sulphur present in solid matrix, which comprises burning a finely divided sulphur-containing sample within a confined combustion chamber, said com-bustion chamber being at a predetermined elevated temperature, continuously removing the combustion gases from the chamber, continuously monitoring the intensity of the infrared spectra for sulphur dioxide in the collected combustion gas as a function of combustion time of the sulphur-containing sample to obtain peaks in the infrared intensity-time pattern indicative of different forms of sulphur and determining from the pattern peaks the quantity of each form of sulphur in the sample.
2. A method according to claim 1 wherein the matrix is coal.
3. A method according to claim 2 wherein the coal sample is placed in the combustion chamber in the form of a uniform, thin layer.
4. A method according to claim 2 wherein the com-bustion chamber is at a temperature in the range of 500°
to 2000°C.
to 2000°C.
5. A method according to claim 1, 2 or 3 wherein the signals from the infrared intensity monitoring are fed to a microprocessor which detects the infrared intensity-time pattern and determines therefrom the quantity of each form of sulphur in the sample.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CA000470308A CA1252705A (en) | 1984-12-17 | 1984-12-17 | Method for analyzing different sulphur forms |
| US07/119,915 US4845040A (en) | 1984-12-17 | 1987-11-13 | Method and apparatus for analyzing different sulphur forms |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CA000470308A CA1252705A (en) | 1984-12-17 | 1984-12-17 | Method for analyzing different sulphur forms |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA1252705A true CA1252705A (en) | 1989-04-18 |
Family
ID=4129391
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA000470308A Expired CA1252705A (en) | 1984-12-17 | 1984-12-17 | Method for analyzing different sulphur forms |
Country Status (2)
| Country | Link |
|---|---|
| US (1) | US4845040A (en) |
| CA (1) | CA1252705A (en) |
Cited By (1)
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|---|---|---|---|---|
| CN109507363A (en) * | 2017-09-15 | 2019-03-22 | 南京麒麟科学仪器集团有限公司 | Raw coal sulfur-bearing quantity measuring method |
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| US5204270A (en) * | 1991-04-29 | 1993-04-20 | Lacount Robert B | Multiple sample characterization of coals and other substances by controlled-atmosphere programmed temperature oxidation |
| US6254828B1 (en) | 1991-04-29 | 2001-07-03 | Lacount Robert B. | Fluid cell substance analysis and calibration methods |
| FR2676280B1 (en) * | 1991-05-10 | 1994-08-05 | Lorraine Laminage | DEVICE FOR MEASURING THE QUANTITY OF A CONSTITUENT CONTAINED IN A SAMPLE OF PRODUCT BURNED IN AN OVEN. |
| US6319717B1 (en) | 1998-07-24 | 2001-11-20 | Lacount Robert B. | Thermal acid base accounting in mine overburden |
| FR2869688B1 (en) * | 2004-04-28 | 2006-07-14 | Inst Francais Du Petrole | METHOD AND DEVICE FOR DETERMINING PETROLEUM CHARACTERISTICS OF GEOLOGICAL SEDIMENTS |
| FR2937737B1 (en) * | 2008-10-29 | 2010-11-12 | Inst Francais Du Petrole | METHOD AND DEVICE FOR RAPID CHARACTERIZATION AND QUANTIFICATION OF SULFUR IN SEDIMENTARY ROCKS AND PETROLEUM PRODUCTS |
| EP2878947A1 (en) * | 2013-12-02 | 2015-06-03 | Geoservices Equipements | Isothermal analysis system and method |
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| CN105277556A (en) * | 2015-11-15 | 2016-01-27 | 常州大学 | Direct-connection linear concurrent sodium hydroxide calibration device in sulfur determinator |
| CN105300985A (en) * | 2015-11-15 | 2016-02-03 | 常州大学 | Gear-driven linear parallel sodium hydroxide calibrating apparatus in sulfur determinator |
| CN105277554A (en) * | 2015-11-15 | 2016-01-27 | 常州大学 | Worm-drive simple sodium hydroxide calibration device in sulfur determinator |
| CN105300982A (en) * | 2015-11-15 | 2016-02-03 | 常州大学 | Gear-driven rotating operation-terminal sodium hydroxide calibration device of sulphur determination device |
| CN105300986A (en) * | 2015-11-15 | 2016-02-03 | 常州大学 | Sodium hydroxide calibrating apparatus of directly connected translation operation terminal in sulfur determinator |
| CN105277546A (en) * | 2015-11-15 | 2016-01-27 | 常州大学 | Direct-connection circular concurrent sodium hydroxide calibration device in sulfur determinator |
| CN105277555A (en) * | 2015-11-15 | 2016-01-27 | 常州大学 | Worm-drive operation-end-translation sodium hydroxide calibration device in sulfur determinator |
| CN105277557A (en) * | 2015-11-15 | 2016-01-27 | 常州大学 | Worm-drive operation-end-rotation sodium hydroxide calibration device in sulfur determinator |
| CN105300983A (en) * | 2015-11-15 | 2016-02-03 | 常州大学 | Gear-driven simple sodium hydroxide calibration device of sulphur determination device |
| CN105277547A (en) * | 2015-11-15 | 2016-01-27 | 常州大学 | Gear-driven double-translational sodium hydroxide calibration device in sulfur determinator |
| CN105300984A (en) * | 2015-11-15 | 2016-02-03 | 常州大学 | Worm wheel-driven circumferentially parallel sodium hydroxide calibration device of sulphur determination device |
| CN105300988A (en) * | 2015-11-15 | 2016-02-03 | 常州大学 | Sodium hydroxide calibration apparatus with direct-connection rotation pedestal in sulfur determination instrument |
| CN105300987A (en) * | 2015-11-15 | 2016-02-03 | 常州大学 | Sodium hydroxide calibration apparatus with worm-transmission rotation pedestal in sulfur determination instrument |
| CN105277549A (en) * | 2015-11-15 | 2016-01-27 | 常州大学 | Gear-driven base-rotation sodium hydroxide calibration device in sulfur determinator |
| CN105277551A (en) * | 2015-11-15 | 2016-01-27 | 常州大学 | Gear drive ring parallel sodium hydroxide calibration device in sulfur determination instrument |
| FR3071063B1 (en) * | 2017-09-12 | 2019-09-13 | IFP Energies Nouvelles | PROCESS FOR THE QUANTIFICATION OF PYRITIC SULFUR AND ORGANIC SULFUR OF A ROCK SAMPLE |
| DE102019120512B4 (en) * | 2019-07-30 | 2021-02-25 | Anton Paar Provetec Gmbh | Flame monitoring for flash point determination or fire point determination |
| CN112683719B (en) * | 2020-11-25 | 2023-07-25 | 中国辐射防护研究院 | Nuclear material ignition accident condition release source item measuring device and evaluation method |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3393051A (en) * | 1965-03-08 | 1968-07-16 | Kerver John Kingsley | Method for determining small concentrations of surface active materials |
| US3904364A (en) * | 1972-02-18 | 1975-09-09 | Nat Res Dev | Methods of and apparatus for determining trace impurities |
| US3847546A (en) * | 1972-10-04 | 1974-11-12 | Chromalytics Corp | Method and system for thermal analysis |
| US3985505A (en) * | 1974-11-21 | 1976-10-12 | Leco Corporation | Combustion system |
| FR2376414A1 (en) * | 1976-12-30 | 1978-07-28 | Inst Francais Du Petrole | METHOD AND DEVICE FOR ANALYSIS OF GEOLOGICAL SEDIMENTS, ENABLING IN PARTICULAR TO DETERMINE THEIR ORGANIC SULFUR CONTENT |
| US4221569A (en) * | 1979-03-01 | 1980-09-09 | Will Ross, Inc. | Chromatographic analysis of gaseous samples containing reactive sulfur |
| US4277368A (en) * | 1980-03-10 | 1981-07-07 | The United States Of America As Represented By The Secretary Of The Navy | Sulfur dioxide detector |
-
1984
- 1984-12-17 CA CA000470308A patent/CA1252705A/en not_active Expired
-
1987
- 1987-11-13 US US07/119,915 patent/US4845040A/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109507363A (en) * | 2017-09-15 | 2019-03-22 | 南京麒麟科学仪器集团有限公司 | Raw coal sulfur-bearing quantity measuring method |
Also Published As
| Publication number | Publication date |
|---|---|
| US4845040A (en) | 1989-07-04 |
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